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Author: Subject: help make white fuming nitric acid.
NeonPulse
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[*] posted on 25-2-2015 at 15:59


Quote: Originally posted by Hawkguy  
Quote: Originally posted by hissingnoise  

If you need water-white HNO3 just add a small pinch of urea as a last resort.

decentn't the resulting Urea nitration cause the release of more NOx, which might be redissolved?


I made a video on the tube called cleaning NO2 from RFNA. It outlines the process I use to get my distilled acid totally clean. Since I don't use a vacuum I fund this necessary for a decent clear acid and it works well.
https://www.youtube.com/watch?v=chGiOsQBlMY

[Edited on 26-2-2015 by NeonPulse]




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greenlight
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[*] posted on 26-2-2015 at 04:47


Thanks for the replies guys, i made a mistake with the type of pump though. It is a ILMvac 400082-03 chemical resistant membrane pump not a diaphragm pump. Its quite hard to find much information on it but it does pull a reasonably good vacuum and boils warm water from the tap when placed under vacuum with it.
Molecular manipulations, I wanted to neutralize the vapours with a basic solution in the dreschel bottle. Will this make damage to the pump minimal considering that it is chemical resistant already?


[Edited on 26-2-2015 by greenlight]
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[*] posted on 26-2-2015 at 06:47


It will certainly help, put so glass wool in the tip of the bubbler to increase the surface area of the bubbles.



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[*] posted on 9-3-2015 at 16:13


Glass wool on the tip of the bubbler tube will not make much of a difference to the efficiency of the scrubber under the given circumstances...trust me. What will make a difference though is mechanical agitation. Put the scrubber onto a magnetic stirrer and add a suitable stirrer bar into the dreschel bottle, that will increase the active neutralising surface area and retention time manyfold and hence also increase the survival chances of your vacuum pump,



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greenlight
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[*] posted on 10-3-2015 at 07:19


Thanks, I will use a Dreschel bottle filled with either a saturated solution of Sodium bicarbonate or Sodium hydroxide base and place the bottle on a magnetic stirrer as well to increase the surface area.
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[*] posted on 16-5-2015 at 12:40


Is is possible to dry about 95% nitric acid to 99% in an desiccator with a normal drying agent.

Because I think I have read somewhere it isn't possible.
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[*] posted on 16-5-2015 at 15:44


Quote: Originally posted by Mr.Greeenix  
Is is possible to dry about 95% nitric acid to 99% in an desiccator with a normal drying agent.

Because I think I have read somewhere it isn't possible.




To dry HNO3 you need to distill it with an equal amount of concentrated sulfuric acid. Preferably under a vaccum. It can't be dried any further in a dessicator. What did you need it for? In most instances 95% will do just fine.




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[*] posted on 17-5-2015 at 05:05


Why it isn't actually possible to dry it in a dessicator? It know that you can dry it by distilling, but it's annoying

I need it for nitrating Glycoluril to the TetraNitro compound with Engagers method.
-> HNO3 + acetic anhydride therefore you really need 99% ?
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[*] posted on 17-5-2015 at 07:15


The concentrated acid has a vapour tension and the vapour contains both water and HNO3...that's why dessicator won't work.
If you understand the concept of distillation plates and negative azeotropic mix, you will understand that below 68% HNO3 it is possible to concentrate HNO3 up to 68% because the vapour is richer at water than the condensed phase; but above 68% the vapour is richer at HNO3 than the condensed phase.

You thus need to catch the water chemically.

[Edited on 17-5-2015 by PHILOU Zrealone]




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[*] posted on 17-5-2015 at 08:03


It is possible to break the azeotrope by adding to the aqueous HNO3 a nitrate salt which is hygroscopic and will form a hydrated salt having greater affinity for the water than does the HNO3. Dehydrated calcium nitrate or magnesium nitrate or anhydrous or nearly anhydrous mixtures of magnesium nitrate with potassium nitrate, sodium nitrate, or ammonium nitrate are useful for breaking the azeotrope of HNO3 and H2O and other anhydrous salts such as zinc nitrate or others may work also.

Some of the nitrates which cannot be dehydrated by baking out the H2O without decomposition to the metal oxides will dehydrate without decomposition when mixed with another nitrate which forms a lower melting point mixture of nitrates, so the water will escape more easily from the melt at a lower temperature. This method avoids the thermal decomposition of a nitrate such as magnesium nitrate which otherwise can't be dehydrated by heat alone. Heating such mixtures under vacuum speeds the dehydration. A complication occurs that some mixtures will form glasses on cooling, instead of crystallizing and crumbling on solidification on cooling, falling apart as loose crystals which are desirable to make easy collection and removal of the dehydrated nitrate salts. Such anhydrous nitrate mixtures are likely also useful in nitration schemes where a solid nitrate is added to sulfuric acid to produce HNO3 as an alternative or in conjunction with using neat HNO3 made separately.
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[*] posted on 15-10-2016 at 12:13
nitric acid of 19.century


I would like to tell something about very old method for to make 100 % HNO3 without destilation.
You have KNO3 + conc. H2SO4 as usually,you can heat it for 70 C,but after you should cold the bottle to 0C .There will crystalised the KO.4SO4.6HO with big long crystals in a good shape.
And you will do this: On the open end of the bottle with freezed crystals you give the second bottle.Now you revers this two bottels and stay it in the easy hand centrifuge and turn it quickly in the hand.The crystals stay in the bottle and the liquid-100% HNO3 is going out to the second bottle.
(Or you can do it with pressure or vacuum)
An because is it without heating and without destillation,it will be free of noxes.
Described by Richard Escales,used by Nobel and I self did it.
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[*] posted on 15-10-2016 at 13:41


Interesting, any original reference? What is KO.4SO4.6HO? Hard to believe any hydrate salts would be formed, in which case the nitric will only be as strong as the starting sulphuric. Wouldn't just potassium bisulfate precipitate, along with a small amount of potassium nitrate? What ratios did you use and did you test the amount of sulfates present in the resulting nitric by dilution and neutralization with calcium carbonate for example?

[Edited on 15-10-2016 by nitro-genes]
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[*] posted on 15-10-2016 at 23:20


It will be better,if I will give here picture of the Book of Escales and you can self read it in original.
The method has two ways.Either 100 % HNO3 or watterless nitration acid (HNO3+H2SO4)My experience is with the watterless nitration acid.And it look like long needles in solid trajectory in all hole of the bottle.The acid flow easy out without moving crystals.
May be it was not 0 C ,I cooled in freezer ,may be it was more cold.
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[*] posted on 16-10-2016 at 02:10




DSCN2452.JPG - 44kB
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Thraxx
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[*] posted on 18-10-2016 at 03:36


yeasterday I did experiment for to explain,if this HNO3 production is possible.I gave 20 g KNO3(1Gewichtteil)
to 38,25 ml H2SO4 /96%/ (3 and 1/2 Gewichtteile).Together was it thick like honey.After one hour was it clear and after them I put it into freezer.After 3 hours was it dense solid substance without crystal needles.Absolute inseparable.
Did I mistake? Yes,befor many years as I did this experiment first time,I took volumen parts not weights parts like Escales wrote.
What now?May be,if I will give there more SA,can it work,but not economical.Unfortunatelly.
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[*] posted on 18-10-2016 at 07:11


Try to heat it for 1 hour or more before putting it in the freezer. KNO3 needs time to fully dissolve, it tends to form lumps in sulfuric acid.
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[*] posted on 18-10-2016 at 09:51


Thank you,I will do. Now I gave 10g KNO3 to 38ml H2SO4.Its a half of "1 Gewichtteil".I freezed and separated (!) big crystals on the bottom of bottle and acid ,better to tell something like thick pink honey.To this pink honey I gave the second half of "1 Gewichtsteil"( =10 g KNO3) Now I will use your advice and will heate and after freeze.
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[*] posted on 19-10-2016 at 03:57


The frozen substance is inseparable,sticky and dense .In other condition,with more liquid part,could it be helpful for lowering of water content in the nitration acid,but the described method by Escales doesnt work.
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[*] posted on 20-10-2016 at 08:50


Allow it to warm to room temp after it sat in the freezer, the crystals will remain! if you have a glass fritted funnel you can remove any smallish crystals that may come over, but they will be inert any ways so not much to be worried about.

Alternatively you can filter with clean fiber glass mating.

if it is gelling bad you have too much water in your acid too bty! Dry Acid can be at -25 and still flow smoothly albeit viscus.
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[*] posted on 20-10-2016 at 10:17


If you have a lot of tiny crystals, then by capillarity the acid may remain stuck to it and forming like a gel.

Also the shape of the crystals has an importance...sometimes needle like crystals intricates into such a mess that it is hard to get the liquid out of it...

--> centrifugation
--> vaccuum filtration
--> extract the anhydrous HNO3 with CH2Cl2




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[*] posted on 20-10-2016 at 10:40


Into the crystal poridge content 20g KNO3 + 38ml H2SO4 I gave 5 g of Sorbitol and 48 hours stooud it out of window without cooling.The acid stood crystalline. Surprisingly was the yield good.The same like with fuming acid.(With the conc. 65%HNO3 is such reaction impossible).
Now I will repeat the experiment. Escales wrote about cooling to 0 C,perhaps was the cooling to quickly and the shape of crystals look it.
(Could be the DCM extract usable for Hexamine nitrolysis? )
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[*] posted on 29-10-2016 at 05:33


This could be an economical way:
1)Mg(NO3)2 x 6 H2O-- heat for to lose the water.It melt at 89 C and destroy at 300 C.Therefore heat between 100- 200 C should be sufficient.
2)Destilation of 300g burned Mg(NO3)2 for each 100 ml HNO3 65%.
3)Over burning of the Mg(NO3)2

(Unfortunatelly it is only my idea now.)
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[*] posted on 31-10-2016 at 06:20


Quote: Originally posted by Thraxx  
This could be an economical way:
1)Mg(NO3)2 x 6 H2O-- heat for to lose the water.It melt at 89 C and destroy at 300 C.Therefore heat between 100- 200 C should be sufficient.
2)Destilation of 300g burned Mg(NO3)2 for each 100 ml HNO3 65%.
3)Over burning of the Mg(NO3)2

(Unfortunatelly it is only my idea now.)

This Mg(NO3)2 process for increasing HNO3 concentration has been covered many times onto the forum. Did you use the forum search engine?




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[*] posted on 31-10-2016 at 06:23


Quote: Originally posted by Thraxx  
Into the crystal poridge content 20g KNO3 + 38ml H2SO4 I gave 5 g of Sorbitol and 48 hours stooud it out of window without cooling.The acid stood crystalline. Surprisingly was the yield good.The same like with fuming acid.(With the conc. 65%HNO3 is such reaction impossible).
Now I will repeat the experiment. Escales wrote about cooling to 0 C,perhaps was the cooling to quickly and the shape of crystals look it.
(Could be the DCM extract usable for Hexamine nitrolysis? )

The initial subject was to make concentrated HNO3, not to make sorbitol hexanitrate.
DCM/HNO3 concentrated may eventually be used for Hexamine nitration...not nitrolysis what means replacing a group (like acetyl or formyl) by a nitro group from HNO3 solvent.




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[*] posted on 31-10-2016 at 07:46


I find this German text a bit strange, as it talks about concentrated sulfuric acid and anhydrous nitrate salts, but describes the salts and the acids produced as being hydrates. The acids are described as either a mix of sulfuric and nitric acid, or in the last sentence as the mono hydrate of nitric acid
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